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Related Concept Videos

¹H NMR of Labile Protons: Temporal Resolution01:10

¹H NMR of Labile Protons: Temporal Resolution

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Protons bonded to heteroatoms such as nitrogen and oxygen exhibit a range of chemical shift values. This is due to the varying degree of hydrogen bonding between the proton and the heteroatom in other molecules. The extent of hydrogen bonding affects the electron density around the proton, thereby giving different chemical shift values for the protons in the proton NMR spectrum.
The –OH proton in alcohols typically appears in the range of δ 2 to 5 ppm but can vary depending on the specific...
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¹H NMR of Labile Protons: Deuterium (²H) Substitution00:48

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This lesson illustrates the role of deuterium substitution in simplifying the NMR spectrum of compounds comprising labile protons. One method employed is the use of deuterium. Amongst the three isotopes of hydrogen, deuterium (2H) has a nucleus composed of one proton and one neutron. When the D2O solvent is added to a pure dry ethanol solution, its labile proton is substituted with deuterium.
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2D NMR: Heteronuclear Single-Quantum Correlation Spectroscopy (HSQC)01:19

2D NMR: Heteronuclear Single-Quantum Correlation Spectroscopy (HSQC)

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Heteronuclear single-quantum correlation spectroscopy (HSQC) is a 2D NMR technique that reveals one-bond correlations between hydrogen and a heteronucleus. The HSQC experiment is similar to the heteronuclear correlation experiment (HETCOR) but is more sensitive. In the HSQC spectrum, the proton chemical shift is plotted on the horizontal F2 axis, while the 13C chemical shift is plotted on the vertical F1 axis. The corresponding proton and 13C spectra are also shown. The HSQC contour plot does...
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¹H NMR of Conformationally Flexible Molecules: Temporal Resolution00:52

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At room temperature, the chair conformer of cyclohexane undergoes rapid ring flipping between two equivalent chair conformers at a rate of approximately 105 times per second. These two chair conformers are in equilibrium. The rapid ring flipping results in the interconversion of the axial proton to an equatorial proton and an equatorial to the axial proton. Such interconversions are too rapid and cannot be detected on the NMR timescale. Hence, the NMR spectrometer cannot distinguish between the...
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2D NMR: Overview of Heteronuclear Correlation Techniques01:18

2D NMR: Overview of Heteronuclear Correlation Techniques

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Heteronuclear correlation spectroscopy is an analytical technique that investigates the coupling between different types of nuclei, often a proton and an X-nucleus, such as carbon-13 or nitrogen-15. This method is commonly used in nuclear magnetic resonance (NMR) spectroscopy to gain insights into complex chemical compounds' structural and compositional aspects. A typical heteronuclear correlation spectrum displays X-nucleus chemical shifts on one axis and a proton spectrum on the other...
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¹H NMR Signal Integration: Overview00:58

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The intensity of a signal, which can be represented by the area under the peak, depends on the number of protons contributing to that signal. The area under each peak is shown as a vertical line called an integral, with the integral value listed under it, as seen in the proton NMR spectrum of benzyl acetate. Each integral value is divided by the smallest integral value to obtain the ratio of the number of protons producing each signal. The ratio reveals the relative number of protons and not...
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Updated: Sep 10, 2025

Quantification of Hydrogen Concentrations in Surface and Interface Layers and Bulk Materials through Depth Profiling with Nuclear Reaction Analysis
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Quantifying Hydrogen Populations in Liquid Mixtures Using 1H NMR Relaxometry.

Pallavi Guha Biswas1, Marc B Taraban1, Katharine T Briggs1

  • 1Bio- and Nano-Technology Center, University of Maryland School of Pharmacy, and Institute for Bioscience and Biotechnology Research, Rockville, Maryland 20850, United States.

Analytical Chemistry
|August 27, 2025
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Summary
This summary is machine-generated.

Time-domain proton nuclear magnetic resonance (¹H NMR) relaxometry quantifies hydrogen populations in liquid mixtures, including drug products. This rapid method accurately determines ingredient fractions, aiding in quality control and content uniformity verification.

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Area of Science:

  • Analytical Chemistry
  • Materials Science
  • Pharmaceutical Science

Background:

  • Liquid mixtures, particularly pharmaceutical products, require precise quantification of components for quality assurance.
  • Traditional analytical methods can be time-consuming and may not fully capture the dynamic nature of liquid mixtures.

Purpose of the Study:

  • To quantify hydrogen population fractions in liquid mixtures, including pharmaceutical formulations, using time-domain ¹H NMR relaxometry.
  • To assess the accuracy and speed of ¹H NMR relaxometry for determining ingredient composition in drug products.
  • To explore the potential of ¹H NMR relaxometry for verifying content uniformity in liquid drug products.

Main Methods:

  • Utilized time-domain proton nuclear magnetic resonance (¹H NMR) relaxometry to measure transverse relaxation rates (R₂(¹H)) of different hydrogen populations.
  • Applied the distinct R₂(¹H) values to differentiate and quantify hydrogen fractions in various liquid mixtures.
  • Analyzed eight diverse drug products, including five emulsions and three solutions.

Main Results:

  • ¹H NMR relaxometry successfully quantified hydrogen population fractions in liquid mixtures within one minute.
  • For drug products with two dominant ingredients, the method provided accurate quantification of hydrogen fractions.
  • Discrepancies between NMR-derived fractions and chemically calculated values were minimal (<2% for seven products, 6% for one).

Conclusions:

  • Time-domain ¹H NMR relaxometry is a rapid and accurate technique for quantifying hydrogen population fractions in liquid mixtures.
  • This NMR approach offers a reliable method for assessing the composition and content uniformity of liquid drug products.
  • The technique holds promise for routine quality control and batch release testing in the pharmaceutical industry.